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This paper reports on Photoluminesceiice (PL) properties of ZnO nanoparticles incorporated in mesoporous silica matrix (MPS). The effect of temperature and annealing times on photoluminescence properties of ZnO/ MPS nanocomposite were studied. The strong UV emission at 363 nm from the sample annealed in oxygen atmosphere at 550°C indicates the formation of very small ZnO nanoparticles. The sample shows blue-green emission band when annealed at 300°C for three hours. The increase in annealing time to 5h turns the blue-green PL band to blue band and further increase in annealing time causes the increase in intensity without any shift. Quenching of blue emission at high temperatures is observed.